Methylhydrazine → 1-Methyl-3-phenyl-1H-pyrazol-5-amine

HRID 402477

反応式

HRID 402477 の反応式
[C:1]([CH2:9][C:10]#[N:11])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:12][NH:13][NH2:14]>CO>[CH3:12][N:13]1[C:10]([NH2:11])=[CH:9][C:1]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[N:14]1

参加物

4

反応物 2

HCID 6061MethylhydrazineHCID 64799Benzoylacetonitrile

生成物 1

HCID 5177791-Methyl-3-phenyl-1H-pyrazol-5-amine収率 71.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of benzoyl acetonitrile (2.0 g, 13.778 mmol) and methyl hydrazine (0.698, 15.156 mmol) in methanol (10 mL) was irradiated under microwave conditions at 110° C. for 90 min. The reaction mixture was cooled to rt and poured into rapidly stirred ice cold water. The obtained solid was collected by filtration, dried under vacuum and triturated with a mixture of pentane-hexane (˜10 mL) to yield a white solid (1.7 g, 71%). [1H-NMR (CDCl3, 300 MHz) δ 7.82-7.65 (m, 2H), 7.45-7.20 (m, 3H), 5.90 (s, 1H), 3.75 (s, 3H), 3.55 (s, 2H); LCMS RtA=0.824 min; [M+H]+=174.1]

後処理

  1. customwas irradiated under microwave conditions at 110° C. for 90 min
  2. additionpoured into rapidly stirred ice cold water
  3. filtrationThe obtained solid was collected by filtration
  4. customdried under vacuum
  5. customtriturated with a mixture of pentane-hexane (˜10 mL)

出典と根拠

ORDレコード
ord-13a444bbc6634ce09bcbd8cf08acef13
出典データセット
uspto-grants-2014_06
特許番号
US08742106B2

関連ノート

読み込み中…